Process of making a reflocculated product



/ portance in example in ghous siliceous materials and eflocculation followed. by reflocculation,

I tions, etc. j

last mentioned purpose Patented To all whom it may concern:

Dec. 1, j

enonen wrnson acnnsom'or CALDWELL,

new mm.

"rnocnss or MAKING A .nnrnoccuna'rnn rnonucr.

it known that I, Gnome WIL8ON AoHnsoN, a citizen of the United States. residing at Caldwell, in the countyv of Essex and State of New J erse have invented certain new and useful mprovements in Processes of Making a Refiocculated Prodnot, of which the following is a specification.

Compositions prepared b sub ecting clay, carbon black, graphite, ful ers earth, amorwith subsequent drying or calcination according to the use for which the product is intended, havev acquired considerable ima number of'arts, being used for the manufacture of crucibles and the like; as fillers for soap, rubber composiand more recently as solid ad sorbents in the refining and decolorization of hydrocarbon oils Certain applications of the product for the are disclosed in my copending applications, Serial Number 7 32,- 112, filed August 14, 1924, and Serial Number 742,429, filed October 8, 1924. The present invention is a simple and relatively inexpensive process 0t makmg such refloocusult that they cuts to 1,456,112, patented Ma lated products.

Certain prior processes of preparing a re flocculated product are disclosed in the pat- E. G. Acheson, Nos. 1,456,111. and 22 1923. As more fully ,explained in t e' aforesaid Patent 1,456,112, the term deflocculation is employed herein to indicate a subdivision of matter brought about through the agency of certain organic bodies known in this art as deflocculating agents. When such deflocculating agents are incorporated with the body to be .deflocculated, the latter in presence of a sufiiciently restricted body otwater or other liquid, and the resulting heavy paste is subjected to prolonged mechanical working, the component particles, or a portion of them, undergo minute masses, are now believed to be ofmolecular dimensions. Such-deflocculated partlcles are be .yond the limits of visibility under ordinary microscopic observation, but appear under the ultra-microscope as brilliant points m intense vibratory movement. Processes of deflocculation and deflocculating agents for the like to] and other bitumens.

son Patent 1,345,306. For English china flocculating mill de'flocculation with the re-' are subdivided into extremely which in some cases at least Appliea tion flled November 22, 1924. Serial No. 751,688.

' use in connection therewith aredisclosed in many prior patents to E. G. Acheson, among whlch may e mentioned U. S. 1,223,350 of April 24, 1017,. as disclosing a preferred mechanical method of effecting the deflocculatlon; U. S. 1,253,556 of January 15, 1918,

"and 1,345,305 or June 29, 1920, as disclosing deflocculatmg agents; and U. S. 1,345,306 of'June 29, 1920, as disclosing the preferred preferred moisture relations, in the defiocculatlng process. However the deflocculation may be accomplished, the deflocculated or colloidal particles may be precipitated from their solution or suspension (refloccu-- lated) by the addition of smallproportions of electrolytes such as hydrochloric acid,

alum or the like. The particles are thereby precipitated n the; form of fragile and porous aggregates, which present enormous sur- .faces relative to their weight. 1

When the reflocculated product :is to be employed as'a solid adsorbent, as for the refining of oils, caloination at high temperatures, of the order of 550-650 C. under strongly oxidizing conditions, and thereafter reduced by crushing, grinding, sieving, etc., to a state of subdivision appropriate for the intended use.

Aecordingto the present invention in its preferred embodiment the desired raw mate it is preferably subjected to rial, as for example china clay or fullers earth, is first subjected to deflocculation under known conditions, as described in the patents to E. G. Acheson above mentioned, the moisture content being maintained, during the deflocculating run, somewhat below the saturation point as disclosed in the Acheclay a moisture content approximating 28% is suitable at this point. 1 I

Under the prior practice it has been-customary to discharge the contents of the deinto water, suspending therein both the defiocculated and non-deflo'eculated portions, and to precipitate the former by addition of electrolyte, the defiocculated particles being precipitated either upon the non-defiocculated particles, or after being floated therefrom, according to the characteristics desired in the product, the reflocculated material being then collected in a filter press. In contradistinction to this, I effect the reflocculation in the same or other mill, while continuing the operation of of about 28%.

attrition, increasing the moisture content asv required to maintain the paste consistency of the charge.

For example, I may proceed as follows in treating English china clay The charge is deflocculated as usual at a moisture content At the conclusion ofthe defiocculating run the moisture content 15 raised slowly to about 40%, whereupon an electrolyte is added and the run continued until the reflocculation is complete. During this latter period the charge continually thickens, provided no further moisture is added. As a modified procedure, I may add the moisture continuously or at intervals during the reflocculation period, under conditions to maintain at all times a suitable Working consistency in the paste.

W'hen reflocculation is complete the paste is removed from the mill and either airdried or ovendried; and is thereafter calcined if desired, the temperature of calcination being appropriate to the particular material used and to the purpose for which it is intended. As a rule calcination is only required when the adsorbent properties of .reflocculation thereof.

the product are to be utilized. The product is then crushed, ground and screened and is ready for use.

I claim 1. Process of making a refiocculated prod uct, comprising subjecting a finely divided solid to successive deflocculation and -reflocculation under attrition.

2. Process of making a refiocculated product, comprising subjecting a finely divided solid in paste form to successive defiocculation and reflocculation under attrition.

3. In a process of making a refiocculated product, the step comprising subjecting a deflocculated material to attrition in presence of an electrolyte, to effect refiocculation thereof.

4. In a product, the step comprising subjecting a deflocculated material in paste form to attrition in presence of an electrolyte, to effect In testimony. whereof, I aflix my signature.

GEORGE WILSON ACHESON.

process of making arefiocculated 

